Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing 1-chloroacetaldehyde oxime

A technology for chloroacetaldehyde oxime and acetaldehyde oxime is applied in the field of preparation of 1-chloroacetaldoxime, which can solve problems such as poor compatibility, explosion of chlorinated products, influence on the yield of chlorination reaction, etc., so as to ensure efficiency and improve yield. The effect of rate and product purity

Pending Publication Date: 2022-04-29
ZHEJIANG JINHUA NEW MATERIALS
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Chlorine gas 1-chloroacetaldoxime can generate by-products such as nitroso compound dimers, and excessive Cl2 will generate 1,1-dichloro-1-nitrosoalkane, and these by-products will affect the yield of chlorination reaction
When the temperature rises slightly, these chlorinated products may explode
[0012] However, 1,3-dialkylimidazolium chloride salt ionic liquid has poor compatibility with acetaldehyde oxime, and its chlorine content is less than 26%, which needs to be further improved to ensure the efficiency of chlorination

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing 1-chloroacetaldehyde oxime
  • Method for preparing 1-chloroacetaldehyde oxime
  • Method for preparing 1-chloroacetaldehyde oxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A method for preparing 1-chloroacetaldoxime, is characterized in that comprising the following steps:

[0040] Put 40g of acetaldehyde oxime into the chlorination kettle after metering, add 150g of chlorinating agent into the chlorination kettle after metering, cool the inside of the kettle with frozen brine, and keep it warm for a certain period of time. At this time, the solution gradually changes from colorless to transparent. Light green, then turn to sea blue, the obtained sea blue transparent solution is 1-chloroacetaldoxime;

[0041] Described chlorinating agent is polychlorinated chlorine addition ionic liquid, and its preparation scheme is as follows:

[0042] S1: Mercapto-Michael addition reaction: under nitrogen atmosphere, add solvent to polytetrafluoroethylene reaction vessel, then add 30g 1-allyl-3-ethylimidazolium chloride salt, stir and add 2g catalyst, then add 20g ( 2-mercaptoethyl)trimethylammonium chloride, stirred and reacted for a certain period o...

Embodiment 2

[0051] A method for preparing 1-chloroacetaldoxime, is characterized in that comprising the following steps:

[0052] Put 45g of acetaldehyde oxime into the chlorination kettle after metering, add 160g of chlorinating agent into the chlorination kettle after metering, cool down the inside of the kettle with frozen brine, and keep it warm for a certain period of time. At this time, the solution gradually changes from colorless to transparent. Light green, then turn to sea blue, the obtained sea blue transparent solution is 1-chloroacetaldoxime;

[0053] Described chlorinating agent is polychlorinated chlorine addition ionic liquid, and its preparation scheme is as follows:

[0054] S1: Mercapto-Michael addition reaction: under nitrogen atmosphere, add solvent to polytetrafluoroethylene reaction vessel, then add 35g 1-allyl-3-ethylimidazolium chloride salt, stir and add 2g catalyst, then add 22g ( 2-mercaptoethyl)trimethylammonium chloride, stirred and reacted for a certain per...

Embodiment 3

[0063] A method for preparing 1-chloroacetaldoxime, is characterized in that comprising the following steps:

[0064] Put 50g of acetaldehyde oxime into the chlorination kettle after metering, add 170g of chlorinating agent into the chlorination kettle after metering, cool the inside of the kettle by passing frozen brine, and keep it warm for a certain period of time. At this time, the solution gradually changes from colorless to transparent. Light green, then turn to sea blue, the obtained sea blue transparent solution is 1-chloroacetaldoxime;

[0065] Described chlorinating agent is polychlorinated chlorine addition ionic liquid, and its preparation scheme is as follows:

[0066] S1: Mercapto-Michael addition reaction: under nitrogen atmosphere, add solvent to polytetrafluoroethylene reaction vessel, then add 40g 1-allyl-3-ethylimidazolium chloride salt, stir and add 3g catalyst, then add 24g ( 2-mercaptoethyl)trimethylammonium chloride, stirred and reacted for a certain pe...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to the technical field of 1-chloroacetaldehyde oxime preparation, in particular to a method for preparing 1-chloroacetaldehyde oxime. According to the method for preparing the 1-chloroacetaldehyde oxime, the polychlorinated chlorine adduct ionic liquid is prepared through the sulfydryl Michael addition reaction, the polychlorinated chlorine adduct ionic liquid is good in compatibility with the acetaldehyde oxime, the chlorine content of the polychlorinated chlorine adduct ionic liquid is larger than 32%, the chlorination efficiency of the acetaldehyde oxime can be further guaranteed, and the yield and the product purity of the 1-chloroacetaldehyde oxime are improved.

Description

technical field [0001] The invention relates to the technical field of 1-chloroacetaldoxime preparation, in particular to a method for preparing 1-chloroacetaldoxime. Background technique [0002] The key to the synthesis of methomyl is the synthesis of the intermediate methomyl oxime. The operation step of the acetaldehyde method is to react acetaldehyde and hydroxylamine hydrochloride under the action of an acid-binding agent, and then react the acetaldehyde oxime with chlorine gas at a certain temperature After a certain period of time, add sodium methyl mercaptide dropwise, adjust the pH value with alkali, cool, filter with suction, and dry. The white crystals obtained are methomyl oxime. [0003] Shi Shenyi et al. disclosed alkylimidazole chloride: a medium for chlorine gas absorption and oxidation reaction, Organic Chemistry, 2021 (31) recorded that l,3-dialkylimidazolium chloride salt ionic liquid was used as a medium for chlorine molecule absorption , the trichlorid...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/12C07C251/38C07D233/60
CPCC07C249/12C07D233/60C07C251/38
Inventor 周强王雄张军良段仲刚张则瑜徐碧涛张超群廖志华
Owner ZHEJIANG JINHUA NEW MATERIALS
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com